You are on page 1of 4

An American National Standard

Designation: D 873 – 02 British Standard 4456

Designation: 138/99

Standard Test Method for


Oxidation Stability of Aviation Fuels (Potential Residue
Method)1
This standard is issued under the fixed designation D 873; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.

This test method has been approved by the sponsoring committees and accepted by the Cooperating Societies in accordance with
established procedures.

This standard has been approved for use by agencies of the Department of Defense.

1. Scope tion Fuels by Laboratory Filtration5


1.1 This test method2 covers the determination of the E 1 Specification for ASTM Thermometers6
tendency of aviation reciprocating, turbine, and jet engine fuels 3. Terminology
to form gum and deposits under accelerated aging conditions.
(Warning—This test method is not intended for determining 3.1 Definitions of Terms Specific to This Standard
the stability of fuel components, particularly those with a high 3.1.1 The following definitions of terms are all expressed in
percentage of low boiling unsaturated compounds, as these terms of milligrams per 100 mL of sample, after “X” hours
may cause explosive conditions within the apparatus.) aging, “X” being the accelerated aging (oxidation) period at
100°C.
NOTE 1—For the measurement of the oxidation stability (induction 3.1.1.1 insoluble gum—deposit adhering to the glass sample
period) of motor gasoline, refer to Test Method D 525.
container after removal of the aged fuel, precipitate, and
1.2 The accepted SI unit of pressure is the kilo pascal (kPa); soluble gum. Insoluble gum is obtained by measuring the
the accepted SI unit of temperature is °C. increase in mass of the glass sample container.
1.3 This standard does not purport to address all of the 3.1.1.2 potential gum—sum of the soluble and insoluble
safety concerns, if any, associated with its use. It is the gum.
responsibility of the user of this standard to establish appro- 3.1.1.3 precipitate—sediment and suspended material in the
priate safety and health practices and determine the applica- aged fuel, obtained by filtering the aged fuel and washings
bility of regulatory limitations prior to use. from the glass sample container.
3.1.1.4 soluble gum—deterioration products present at the
2. Referenced Documents end of a specific aging period. These deterioration products
2.1 ASTM Standards: exist in solution in the aged fuel and as the toluene-acetone
D 381 Test Method for Existent Gum in Fuels by Jet soluble portion of the deposit on the glass sample container.
Evaporation3 The soluble gum is obtained as a nonvolatile residue by
D 525 Test Method for Oxidation Stability of Gasoline evaporating the aged fuel and the toluene-acetone washings
(Induction Period Method)3 from the glass sample container.
D 4057 Practice for Manual Sampling of Petroleum and 3.1.1.5 total potential residue—sum of the potential gum
Petroleum Products4 and the precipitate.
D 5452 Test Method for Particulate Contamination in Avia-
4. Summary of Test Method
4.1 The fuel is oxidized under prescribed conditions in a
1
This test method is under the jurisdiction of ASTM Committee D02 on pressure vessel filled with oxygen. The amounts of soluble
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee gum, insoluble gum, and precipitate formed are weighed.
D02.14 on Stability and Cleanliness of Liquid Fuels.
(Warning—In addition to other precautions, to provide pro-
Current edition approved Dec. 10, 2002. Published March 2003. Originally
approved in 1946. Last previous edition approved in 1999 as D 873–99a. tection against the possibility of explosive rupture of the
2
Further information can be found in the June 1978, January 1979, and June
1986 editions of the Institute of Petroleum Review.
3 5
Annual Book of ASTM Standards, Vol 05.01. Annual Book of ASTM Standards, Vol 05.03.
4 6
Annual Book of ASTM Standards, Vol 05.02. Annual Book of ASTM Standards, Vol 14.03.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

1
D 873 – 02
pressure vessel, the pressure vessel should be operated behind 7.2 Oxygen, commercially available extra dry oxygen of not
an appropriate safety shield.) less than 99.6 % purity.
5. Significance and Use 8. Sampling
5.1 The results (of these tests) can be used to indicate
8.1 Sample in accordance with the procedure for oxidation
storage stability of these fuels. The tendency of fuels to form
stability, as described in Practice D 4057.
gum and deposits in these tests has not been correlated with
field performance (and can vary markedly) with the formation
9. Preparation of Apparatus
of gum and deposits under different storage conditions.
9.1 Thoroughly clean a glass sample container to remove
6. Apparatus traces of any adhering material. Immerse the container and its
6.1 Oxidation Pressure Vessel, Burst Disc Assembly, Glass cover in a mildly alkaline or neutral pH laboratory detergent
Sample Container and Cover, Accessories and Pressure Gage, cleaning solution. The type of detergent and conditions for its
as described in the Annex to Test Method D 525. (Warning— use need to be established in each laboratory. The criterion for
Provision shall be made to safely vent any expelled gases or satisfactory cleaning shall be a matching of the quality of that
flames away from the operator, other personnel, or flammable obtained with chromic acid cleaning solutions (or some other
materials as a safety precaution if the burst-disc ruptures.) equivalently strong oxidizing non-chromium containing acid
cleaning solutions) on used sample containers and covers
NOTE 2—Pressure vessels conforming to Test Method D 525/1980 are
also suitable, but the specified burst-disc shall be attached. The burst disc
(fresh chromic acid, 6-h soaking period, rinsing with distilled
assembly shall be mechanically designed to ensure that it cannot be water and drying). For this comparison, visual appearance and
incorrectly fitted. mass loss on heating the glassware under test conditions may
be used. Detergent cleaning avoids the potential hazards and
6.2 Thermometer, having a range as shown below and
inconveniences related to the handling of highly corrosive and
conforming to the requirements as prescribed in Specification
strongly oxidizing acid solutions; this procedure remains the
E 1, or specifications for IP thermometers:
reference cleaning practice and, as such, may function as an
Thermometer Range Thermometer Number
ASTM IP alternate to the preferred procedure, cleaning with detergent
95 to 103°C 22C 24C solutions. Remove from the cleaning solution by means of
NOTE 3—Other temperature sensing devices that cover the temperature corrosion-resistant steel forceps and handle only with forceps
range of interest, such as thermocouples or platinum resistance thermom- thereafter. Wash thoroughly first with tap water and then with
eters, that can provide equivalent or better accuracy and precision, may be deionized or distilled water, and dry in an oven at 100 to 150°C
used in place of the thermometers specified in 6.2. for 1 h. Cool the sample containers and covers for at least 2 h
6.3 Drying Oven, air oven maintained at 100 to 150°C. in the cooling vessel in the vicinity of the balance. Weigh to the
6.4 Forceps, corrosion-resistant, steel. nearest 0.1 mg, and record mass.
6.5 Filtering Crucible, sintered-glass, fine porosity. 9.1.1 Experience indicates that the amount of insoluble gum
6.6 Oxidation Bath, as described in the Annex to Test is negligible in aviation reciprocating engine fuels. Therefore,
Method D 525. The liquid shall be water or a mixture of the glass sample container need not be weighed when testing
ethylene glycol and water, as required. The temperature can be such fuels unless visible evidence of insoluble matter remains
controlled thermostatically at 100 6 0.2°C, or by maintaining in the container after treatment with gum solvent. In such
it at its boiling point, which must be between 99.5 to 100.5°C. cases, the test must be repeated and the mass of the container
If a liquid medium other than water is used, an appropriate recorded.
mechanical stirrer/mixer shall be used to maintain uniformity 9.2 Drain any fuel from the pressure vessel and wipe the
of the liquid bath at 100 6 0.2°C. A non self-resettable device inside of the pressure vessel and pressure vessel closure, first
shall be fitted on all new baths to ensure that the heater is with a clean cloth moistened with gum solvent and then with a
switched off if the liquid bath falls below a safe level. Users of clean, dry cloth. Remove the filler rod from the stem, and
older baths without this device are strongly urged to have the carefully clean any gum or fuel from the stem, rod, and needle
equipment retrofitted to ensure safe operation. valve with gum solvent. The pressure vessel, the valve, and all
connecting lines shall be thoroughly dry before each test is
NOTE 4—Electric heating blocks are known to be used. These blocks
can have heating capacities, heating rates, and heat transfer characteristics
started. (Warning—Volatile peroxides, which may have
that differ from those of a liquid bath. An electric heating block may be formed during a previous test, may accumulate in the equip-
used in place of the liquid bath as long as the sample heating rate and ment, producing a potentially explosive environment. Special
sample temperature are demonstrated to be equivalent to that of the liquid care in cleaning after each test is needed to ensure that the filler
bath. rod, stem, and needle valve are free of these peroxides.)
6.7 Cooling Vessel—A desiccator or other type of tightly 9.3 If a thermostatically controlled constant temperature
covered vessel for cooling the beakers before weighing. The oxidation bath is used, adjust the temperature to 100 6 0.1°C
use of a drying agent is not recommended. and maintain it within this temperature range for the duration
of the test.
7. Reagents and Materials 9.4 If a boiling water oxidation bath is used, adjust the
7.1 Gum Solvent—A mixture of equal volumes of toluene temperature within the range from 99.5 to 100.5°C by the
and acetone. addition of water or a higher boiling liquid such as ethylene

2
D 873 – 02
glycol. Factors are given in Table 1 to adjust the “X” hour aging remove any gum. Mix the oxidized fuel and rinses thoroughly,
time if the bath temperature at the start of the test deviates from and preserve the mixture for the determination of soluble gum.
100°C. Proceed with the test as specified in 10.6. If a precipitate is
observed, and if the amount is required by specifications,
10. Procedure determine the initial mass of the filtering crucible (see 6.5) that
10.1 Bring the pressure vessel and the fuel to be tested to a is to be used and filter the oxidized fuel through the crucible
temperature from 15 to 25°C. Place the weighed glass sample and save the filtrate. A vacuum filtration set-up has been found
container in the pressure vessel and add 100 6 1 mL of test suitable to use, although precautions should be taken to avoid
specimen. Alternatively, transfer 100 6 1 mL of sample into the potential of static discharges, such as described in Test
the weighed glass sample container first, before placing the Method D 5452. Wash the interior of the glass container twice
glass sample container into the pressure vessel. Cover the same with 10-mL portions of gum solvent to remove any gum or
container, close the pressure vessel, and using a quick release precipitate. Filter the washings through the crucible, adding
coupling, introduce oxygen until a pressure from 690 to 705 them to the oxidized fuel filtrate, and mix thoroughly. Preserve
kPa is attained. Allow the gas in the pressure vessel to escape the mixture for the determination of soluble gum.
slowly through the needle valve at a rate not to exceed 345 10.5 Dry the crucible in an oven maintained at 100 to 150°C
kPa/min. Repeat the charging and exhausting of the oxygen
for at least 1 h, cool in a cooling vessel to approximately room
once more in order to flush out the air originally present.
temperature (for at least 2 h), and weigh the crucible (that is,
Introduce oxygen again until a pressure of from 690 to 705 kPa
the crucible plus residue) to determine its final mass. Subtract
is attained and observe for leaks, ignoring an initial rapid drop
the initial mass of the crucible from the final mass of the
in pressure (generally not over 40 kPa), which can be observed
crucible. Record any increase in mass as precipitate, A.
because of the solution of oxygen in the sample. Assume the
absence of leaks, and proceed with the test if the rate of 10.6 Dry the glass sample container in an oven maintained
pressure drop does not exceed 15 kPa in 10 min. at 100 to 150°C for 1 h, cool in a cooling vessel, and weigh.
10.2 Place the charged pressure vessel in one of the de- Two hours has been found to be a suitable time to cool the glass
scribed oxidation baths, being careful to avoid shaking, and sample container. Record any increase in mass as insoluble
record the time of immersion as the starting time. Leave the gum, B.
pressure vessel in the oxidation bath for the specified “X” hour 10.7 Divide the mixture obtained in 10.4 into two equal
aging time. If the temperature at the start of a test varies from portions (within 2 mL), and determine the soluble gum existing
100°C, adjust the “X” hour aging time by the correction factors therein by the procedure and test conditions described in Test
given in Table 1. Method D 381, using in each test the entire half portion instead
10.3 At the completion of the period of oxidation, remove of the 50-mL test specimen specified in Test Method D 381.
the pressure vessel from the bath. To minimize further oxida- Record the sum of the increase in mass of the two beakers as
tion of the test specimen and to provide for safe venting of the soluble gum, C, as calculated in accordance with the following
pressure vessel, cool the pressure vessel to approximately room equation:
temperature within 30 min after removal from the bath, using C 5 1000 3 ~~D2E! 1 ~F2G! 1 2~X2Y!! (1)
water #35°C. Release the pressure slowly through the needle
valve at a rate not to exceed 345 kPa/min. Take the pressure where:
vessel apart, and remove the sample container. C = soluble gum, mg/100 mL,
10.4 Transfer the oxidized fuel from the glass sample D = mass of test specimen beaker 1 + residue, g,
container to a graduated flask, such as a graduated, stoppered E = mass of test specimen beaker 1, g,
cylinder, that will allow mixing of approximately 120 mL, if no F = mass of test specimen beaker 2 + residue, g,
visible precipitate is observed or if the amount is not specifi- G = mass of test specimen beaker 2, g,
cally required by specifications. Wash the interior of the glass X = mass of tare beaker (before), g, and
sample container twice with 10-mL portions of gum solvent to Y = mass of tare beaker (after), g.

11. Report
TABLE 1 Aging Time Correction Factors

NOTE—To obtain the correct aging time at the operating temperature,


11.1 Calculate the results obtained by combining the sepa-
multiply the time specified for 100°C by the correction factor. rately determined residues as prescribed in Table 2 and report
Temperature,°C Correction Factor
as “X” hour aging characteristics, Test Method D 873 as x
mg/100 mL or < 1mg/100 mL.
99.5 1.06
99.6 1.04
99.7 1.03 12. Precision and Bias
99.8 1.02
99.9 1.01 12.1 The precision of the test method as determined by the
100.0 1.00 statistical examination of interlaboratory test results is as
100.1 0.99
100.2 0.98 follows:
100.3 0.97 12.1.1 Repeatability—The difference between successive
100.4 0.96
100.5 0.95 results obtained by the same operator with the same apparatus
under constant operating conditions on identical test material

3
D 873 – 02
TABLE 2 Aging Characteristics
Residue Fractions to be Combined
Aging Characteristic to be Reported
Aviation Reciprocating Engine Fuel Aviation Turbine Fuel
Potential gum, mg/100 mL sum of insoluble gum and soluble gum (B + C) ...
Precipitate, mg/100 mL precipitate (A) if required ...
Total potential residue, mg/100 mL ... sum of precipitate A (if required) insoluble gum
B and soluble gum C (A + B + C)

would, in the long run, in the normal and correct operation of Reproducibility (16 h aging)
the test method, exceed the following values only in one case Aviation Reciprocat- Aviation Turbine Fuel
ing Engine Fuel
in twenty: Potential
Repeatability (16 h aging) Gum, mg/100 mL
Aviation Recipro- Aviation Turbine Up to 5 3 4
cating Engine Fuel Fuel Over 5 to 10 4 5
Potential Over 10 to 20 6 7
Gum, mg/100 mL Precipitate, mg/100 mL
Up to 5 2 2 Up to 2 1
Over 5 to 10 3 3
Over 10 to 20 4 5 12.2 Bias—Since there is no accepted reference material
Precipitate, mg/100 mL available for determining the bias for the procedure in Test
Up to 2 1
Method D 873 for measuring oxidation stability, bias has not
12.1.2 Reproducibility—The difference between two single been determined.
and independent results obtained by different operators work-
ing in different laboratories on identical test material would, in 13. Keywords
the long run, exceed the following values only in one case in 13.1 aviation fuels; gum (insoluble, soluble, potential);
twenty: oxidation stability; potential residue; total potential residue

SUMMARY OF CHANGES

Committee D02.14 has identified the location of selected changes to this standard since the last issue
(D 873–99a) that may impact the use of this standard.

(1) Added Test Method D 5452 to Section 2, Referenced 10.5. Identified a suitable filtration set-up that could be used
Documents. and alerted users of a potential safety concern.
(2) Updated 10.4 to explicitly state that an initial mass of the (3) Updated 10.5 regarding the drying time and the precipitate
filtering crucible is needed when a precipitate is observed in calculation.
order to determine the increase in mass of the precipitate in

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org).

You might also like